CN113387697A - Sodium bismuth titanate-based ceramic material with high ferroelectric stability, ultra-fast charge and discharge and high energy storage efficiency and preparation method thereof - Google Patents
Sodium bismuth titanate-based ceramic material with high ferroelectric stability, ultra-fast charge and discharge and high energy storage efficiency and preparation method thereof Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 48
- 238000004146 energy storage Methods 0.000 title claims abstract description 29
- FSAJRXGMUISOIW-UHFFFAOYSA-N bismuth sodium Chemical compound [Na].[Bi] FSAJRXGMUISOIW-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 229910002115 bismuth titanate Inorganic materials 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000000919 ceramic Substances 0.000 claims abstract description 19
- 238000005245 sintering Methods 0.000 claims abstract description 18
- 238000000498 ball milling Methods 0.000 claims abstract description 16
- 239000011734 sodium Substances 0.000 claims abstract description 12
- 230000010287 polarization Effects 0.000 claims abstract description 11
- 229910002971 CaTiO3 Inorganic materials 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 18
- 238000000227 grinding Methods 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 16
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 12
- 229910052726 zirconium Inorganic materials 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000004570 mortar (masonry) Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- 239000004677 Nylon Substances 0.000 claims description 6
- 229920001778 nylon Polymers 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 230000015556 catabolic process Effects 0.000 claims description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 4
- 238000009694 cold isostatic pressing Methods 0.000 claims description 3
- 238000010304 firing Methods 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000012856 weighed raw material Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 2
- 239000010453 quartz Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000001351 cycling effect Effects 0.000 abstract description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 10
- 238000012360 testing method Methods 0.000 description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 description 4
- 239000011232 storage material Substances 0.000 description 4
- 229910010252 TiO3 Inorganic materials 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 229910052737 gold Inorganic materials 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 238000001757 thermogravimetry curve Methods 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229910001651 emery Inorganic materials 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 238000001683 neutron diffraction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
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- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/46—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates
- C04B35/462—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates
- C04B35/475—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on titanium oxides or titanates based on titanates based on bismuth titanates
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Abstract
The invention discloses a sodium bismuth titanate-based ceramic material with high ferroelectric stability, ultra-fast charge and discharge and high energy storage efficiency and a preparation method thereof, wherein the general formula of the ceramic material is (1-x) Na0.5Bi0.5TiO3‑xCaTiO3In which x represents CaTiO3The molar ratio of the x to the total mass is 0.1-0.25. The ceramic material is prepared by the process steps of material preparation, pre-sintering, ball milling, tabletting, pressureless closed sintering and the like. The preparation method is simple, the repeatability is good, the yield is high, the obtained ceramic material has high ferroelectric stability (frequency stability and cycling stability), extremely low remanent polarization, extremely high energy storage efficiency and charge-discharge performance, strong practicability and easy production, is a lead-free ferroelectric ceramic with excellent performance, and is a novel alternative material in the field of pulse power material systems.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to a sodium bismuth titanate-based ceramic material with high ferroelectric stability, ultra-fast charge and discharge and high energy storage efficiency and a preparation method thereof.
Background
With the development of social production, the problems of high pollution, low efficiency and reserves brought by the traditional fossil energy sources are not ignored. Therefore, it is crucial to develop a clean energy storage material with no pollution and high efficiency. In the electronic industry, energy storage ceramic materials have exhibited excellent market value and economic benefits. The method is widely applied to the fields of sensors, instrument capacitors and the like. However, most of the conventional energy storage ceramics are based on lead (Pb) and may cause harm to human bodies during use. Therefore, the use of lead-containing related electronic components has been controlled or prohibited in international standards. Based on this, many scholars have been respectively put into the research of lead-free energy storage materials, wherein, in 1960, Smolenskii et al synthesized Na for the first time0.5Bi0.5TiO3(BNT) having a crystal structure typical of perovskite structure. Since Bi3+With Pb2+Is the same and is considered to be the best candidate material for replacing the lead-containing ceramic. A site is composed of Bi3+And Na+Co-occupied with the B site being Ti4+Wherein the coordination number of the A site ion is 12 and the coordination number of the B site ion is 6. In recent years, more scholars agree with the theory of relaxation ferroelectrics of BNT ceramics, and Suchancz et al provide data support for the theory through a series of test methods such as neutron diffraction, XRD, temperature-changing P-E curves and the like. Pure BNT, although having high saturation polarization, has high remanent polarization and high conductivity, which severely limits its development in the direction of energy storage. Meanwhile, the ferroelectric stability of the ferroelectric ceramic is also an important index for evaluating the performance of the ferroelectric ceramic, and the original full and complete electric hysteresis loop of the material is difficult to maintain after the ferroelectric ceramic is repeatedly applied with an electric field. Therefore, good ferroelectric stability is an important problem to be solved by in the practical application field of the ferroelectric ceramic capacitor. In addition, the key problem of improving the energy storage efficiency is to reduce the residual polarization intensity of BNT and obtain a slender electric hysteresis loop. In 2018, Li et al succeeded in Sr relaxor ferroelectric0.7Bi0.2TiO3Introduction into BNT to prepare bulk ceramic and multilayer ceramic, Sr2+The long-range order of BNT ceramic dipole is destroyed by doping ions, and polar nano is generatedAnd in a micro area, 80% of energy storage efficiency is finally obtained.
At present, it is still difficult to obtain ceramic energy storage materials with high frequency stability, fatigue resistance stability, and high energy storage density and energy storage efficiency at the same time. Therefore, the development of a material with high energy storage density, high energy storage efficiency and excellent stability is a key objective for preparing energy storage materials.
Disclosure of Invention
The invention aims to provide a sodium bismuth titanate-based ceramic material with high ferroelectric stability, ultra-fast charge and discharge and extremely high energy storage efficiency, and a preparation method for the ceramic material.
For the above purpose, the ceramic material of the present invention has the general formula (1-x) Na0.5Bi0.5TiO3-xCaTiO3In which x represents CaTiO3The molar ratio of x to the total mass is 0.1-0.25; the ceramic is of a pure perovskite structure, the dielectric breakdown field strength is 140-160 kV/cm, and the polarization strength is 18.4-20.1 mu C/cm2The residual polarization intensity is 0.4-2.1 μ C/cm2。
In the general formula, the preferable value of x is 0.2, the ceramic material is of a rhombohedral phase R3C pure perovskite structure, the dielectric breakdown strength is 160kV/cm, and the polarization strength is 19.8 mu C/cm2The energy storage density is 1.26J/cm3The energy storage efficiency is 91.3%, the performance is stable within the frequency range of 10-500 Hz, and the performance is stable after 1-10000 times of circulation.
The preparation method of the bismuth sodium titanate-based ceramic material comprises the following steps:
1. ingredients
According to (1-x) Na0.5Bi0.5TiO3-xCaTiO3Respectively weighing TiO with the purity of 98%2CaCO of 99% purity3Bi with a purity of 98.9%2O3Na with a purity of 99.8%2CO3(ii) a Uniformly mixing all the weighed raw materials, putting the mixture into a nylon tank, fully mixing and ball-milling the mixture for 18 to 24 hours by taking zirconium balls as grinding balls and absolute ethyl alcohol as a ball-milling medium, separating the zirconium balls, and drying the mixture of the raw materials at the temperature of between 80 and 100 ℃ for 24 to 36And grinding the mixture by using a mortar, and sieving the mixture by using a sieve of 80-100 meshes.
2. Pre-firing
And (3) placing the raw material mixture obtained in the step (1) into a quartz crucible, compacting by using a grinding rod, covering, presintering for 3-4 hours at 850-900 ℃, naturally cooling to room temperature, and grinding by using a mortar to obtain the presintering powder.
3. Secondary ball milling
Putting the pre-sintering powder into a nylon tank, taking zirconium balls as grinding balls and absolute ethyl alcohol as a ball milling medium, fully mixing and ball milling for 18-24 hours, separating the zirconium balls, drying the pre-sintering powder for 24-36 hours at 80-100 ℃, grinding by using a mortar, and sieving by using a 180-200-mesh sieve.
4. Tabletting
And pressing the pre-sintering powder sieved by the 180-200-mesh sieve into a cylindrical blank by using a powder tablet press, and then carrying out cold isostatic pressing for 15-20 minutes under the pressure of 200-300 MPa.
5. Pressureless closed sintering
And (3) placing the cylindrical blank on a zirconium oxide flat plate, placing the zirconium oxide flat plate in an alumina closed sagger, heating to 1160-1190 ℃ at the speed of 2-5 ℃/min, sintering for 1.5-3 hours, and naturally cooling to room temperature along with a furnace to prepare the sodium bismuth titanate-based ceramic material.
The invention has the following beneficial effects:
the preparation method is simple, the repeatability is good, the yield is high, the obtained ceramic material has high ferroelectric stability (frequency stability and cycling stability), extremely low remanent polarization, extremely high energy storage efficiency and charge-discharge performance, strong practicability and easy production, is a lead-free ferroelectric ceramic with excellent performance, and is a novel alternative material in the field of pulse power material systems.
Drawings
FIG. 1 is an XRD pattern of the sodium bismuth titanate-based ceramic material prepared in examples 1 to 4.
FIG. 2 is a dielectric thermogram of the sodium bismuth titanate-based ceramic material prepared in examples 1 to 4.
Fig. 3 is a unipolar P-E hysteresis plot of the sodium bismuth titanate-based ceramic material prepared in example 3.
Fig. 4 is a graph of the frequency stability P-E hysteresis loop of the sodium bismuth titanate-based ceramic material prepared in example 3.
Fig. 5 is a graph of the cycle stability P-E hysteresis loop of the sodium bismuth titanate-based ceramic material prepared in example 3.
Fig. 6 is an underdamped pulsed discharge plot of the sodium bismuth titanate-based ceramic material prepared in example 3.
FIG. 7 is a discharge diagram of an over-damped pulse of the sodium bismuth titanate-based ceramic material prepared in example 3, with the inset being a discharge response time diagram.
Detailed Description
The invention will be further described in detail with reference to the following figures and examples, but the scope of the invention is not limited to these examples.
Example 1
1. Ingredients
According to 0.9Na0.5Bi0.5TiO3-0.1CaTiO3Respectively weighing TiO with the purity of 98%27.359g of 99% pure CaCO30.912g of Bi with a purity of 98.9%2O39.571g of Na with a purity of 99.8%2CO32.157 g; mixing all the weighed raw materials uniformly, putting the mixture into a nylon tank, taking zirconium balls as grinding balls and absolute ethyl alcohol as a ball milling medium, wherein the mass ratio of the absolute ethyl alcohol to the raw material mixture is 1:1.2, performing ball milling for 24 hours at 401 rpm by using a ball mill, separating the zirconium balls, putting the raw material mixture into a drying oven, drying for 24 hours at 80 ℃, grinding for 30 minutes by using a mortar, and sieving by using an 80-mesh sieve.
2. Pre-firing
And (2) placing the raw material mixture which is sieved by the sieve with 80 meshes in the step (1) into an alumina crucible, compacting by using an agate rod, covering, placing into a resistance furnace, heating to 900 ℃ at the heating rate of 3 ℃/min for presintering for 3 hours, naturally cooling to room temperature, discharging, and grinding for 10 minutes by using a mortar to obtain the presintering powder.
3. Secondary ball milling
Putting the pre-sintered powder into a nylon tank, taking zirconium balls as grinding balls and absolute ethyl alcohol as a ball milling medium, wherein the mass ratio of the absolute ethyl alcohol to the pre-sintered powder is 1:1.2, ball milling for 24 hours at 401 r/min by using a ball mill, separating the zirconium balls, drying the pre-sintered powder in a drying oven for 24 hours at 80 ℃, grinding for 10 minutes by using a mortar, and sieving by using a 180-mesh sieve.
4. Tabletting
The pre-sintered powder after passing through the 180 mesh sieve was pressed into a cylindrical blank having a diameter of 11.5mm and a thickness of 0.8mm by a powder tablet press, and then subjected to cold isostatic pressing under a pressure of 200MPa for 10 minutes.
5. Pressureless closed sintering
Placing the cylindrical blank on a zirconia flat plate, placing the zirconia flat plate in an alumina closed sagger, heating to 1160 ℃ at the speed of 3 ℃/min, sintering for 3 hours, naturally cooling to room temperature along with a furnace, and preparing the powder with the molecular formula of 0.9Na0.5Bi0.5TiO3-0.1CaTiO3The bismuth sodium titanate-based ceramic material.
Example 2
In step 1 of this example, 0.85Na was used0.5Bi0.5TiO3-0.15CaTiO3Respectively weighing TiO with the purity of 98%27.431g of 99% pure CaCO31.383g of Bi with a purity of 98.9%2O39.129g of Na with a purity of 99.8%2CO32.058 g; and step 5, placing the zirconia flat plate in an alumina closed sagger, heating to 1170 ℃ at the speed of 3 ℃/min, sintering for 3 hours, and naturally cooling to room temperature along with the furnace. The other steps were the same as in example 1, and a preparation having a molecular formula of 0.85Na0.5Bi0.5TiO3-0.15CaTiO3The bismuth sodium titanate-based ceramic material.
Example 3
In step 1 of this example, as 0.8Na0.5Bi0.5TiO30.2CaTiO3Respectively weighing TiO with the purity of 98%27.505g of 99% pure CaCO31.862g of Bi with a purity of 98.9%2O38.677g of Na with a purity of 99.8%2CO31.956 g; step 5, placing the zirconia flat plate in an alumina closed sagger, heating to 1180 ℃ at the rate of 3 ℃/minute, sintering for 3 hours, and naturally cooling to room temperature along with the furnace. The other steps were the same as in example 1, and a preparation having a molecular formula of 0.8Na was made0.5Bi0.5TiO3-0.2CaTiO3The bismuth sodium titanate-based ceramic material.
Example 4
In step 1 of this example, 0.75Na was used0.5Bi0.5TiO3-0.25CaTiO3Respectively weighing TiO with the purity of 98%27.580g of 99% pure CaCO32.351g of Bi with a purity of 98.9%2O38.217g of Na with a purity of 99.8%2CO31.852 g; and step 5, placing the zirconia flat plate in an alumina closed sagger, heating to 1190 ℃ at the speed of 3 ℃/min, sintering for 3 hours, and naturally cooling to room temperature along with the furnace. The other steps were the same as in example 1, and a preparation having a molecular formula of 0.75Na was made0.5Bi0.5TiO3-0.25CaTiO3The bismuth sodium titanate-based ceramic material.
One of the surfaces of the ceramic materials prepared in the above examples 1 to 4 was selected and ground by 320 mesh sandpaper, then ground by 800 mesh sandpaper, and finally polished to a thickness of 0.5mm by 1500 mesh sandpaper and emery, and then ground into powder after being wiped clean by alcohol ultrasound, and then XRD test was performed by using a Japanese MiniFlex600 type diffractometer, and the result is shown in FIG. 1. Polishing the ceramic material prepared in the embodiment 1-4, coating silver electrodes with the thickness of 0.02mm on the upper and lower surfaces of the ceramic, placing the ceramic in a resistance furnace at 840 ℃ for 30 minutes, naturally cooling the ceramic to room temperature, and testing the change relationship between the dielectric constant and the loss of the material with the temperature under different frequencies by using an Agilent E4980A type dielectric temperature spectrometer, wherein the result is shown in FIG. 2. After polishing the ceramic material prepared in example 3, gold electrodes with a thickness of 0.02mm and a diameter of 2mm were coated on the upper and lower surfaces of the ceramic material, and a ferroelectric performance test, a unipolar P-E hysteresis loop, and a frequency stability test were performed using an aixact ct-TF2000 model ferroelectric parameter tester, and the results are shown in fig. 3 to 5. After polishing the ceramic material prepared in example 3, gold electrodes with a thickness of 0.02mm and a diameter of 2mm were coated on the upper and lower surfaces of the ceramic, and a charge and discharge test was performed using a CFD-001go Instruments capacitance charge and discharge system, with an over-damping resistance value of 200 Ω, and the test results are shown in fig. 6 to 7.
As can be seen from FIG. 1, the ceramic materials prepared in examples 1 to 4 are all pure perovskite structures, and always maintain the R3c rhombohedral phase. Fig. 2 shows the dielectric thermograms of the ceramic materials prepared in examples 1 to 4, in which the dielectric constant variation behavior of the ceramic materials with the temperature variation is marked, and as the CT doping amount increases, the curie temperature of the materials gradually moves to a low temperature, the relaxation behavior of the materials becomes more obvious, and the dielectric temperature stability gradually becomes better. The test result of FIG. 3 shows that the ceramic material of example 3 has extremely high energy storage efficiency, which is as high as 91.3%, and has high energy storage density of 1.26J/cm3. The test result of fig. 4 shows that the ceramic material of example 3 still maintains a good and complete hysteresis loop in a wide frequency range, which indicates that the ceramic material has very high frequency stability in the frequency range of 10 to 500 Hz. The results in fig. 5 show that the ceramic material of example 3 still maintains a good and complete hysteresis loop without difference change in the multi-cycle test range, which indicates that the ceramic material has very high cycle stability in the test range of 1-10000 times. As can be seen from FIGS. 6 and 7, the ceramic material of example 3 has extremely high current density and power density, respectively, of 1520A/cm at a low electric field of 150kV/cm2、115MW/cm3And simultaneously has extremely fast charge-discharge response time of 94.8 ns. Therefore, the ceramic material has good ferroelectric stability, high pulse power performance and extremely high energy storage efficiency, and is a lead-free ferroelectric ceramic with excellent performance.
Claims (3)
1. A sodium bismuth titanate-based ceramic material with high ferroelectric stability, ultra-fast charge and discharge and high energy storage efficiency is characterized in that: the general formula of the ceramic material is (1-x) Na0.5Bi0.5TiO3-xCaTiO3In which x represents CaTiO3The molar ratio of x to the total mass is 0.1-0.25; the ceramic is of a pure perovskite structure, the dielectric breakdown field strength is 140-160 kV/cm, and the polarization strength is 18.4-20.1 mu C/cm2The residual polarization intensity is 0.4-2.1 μ C/cm2。
2. According to the rightThe sodium bismuth titanate-based ceramic material with high ferroelectric stability, ultra-fast charge and discharge and high energy storage efficiency as claimed in claim 1, characterized in that: the value of x is 0.2, the ceramic material is of a rhombohedral phase R3C pure perovskite structure, the dielectric breakdown strength is 160kV/cm, and the polarization strength is 19.8 mu C/cm2The energy storage density is 1.26J/cm3The energy storage efficiency is 91.3%, the performance is stable within the frequency range of 10-500 Hz, and the performance is stable after 1-10000 times of circulation.
3. A method for preparing a sodium bismuth titanate-based ceramic material according to claim 1, which comprises the following steps:
(1) ingredients
According to (1-x) Na0.5Bi0.5TiO3-xCaTiO3Respectively weighing TiO with the purity of 98%2CaCO of 99% purity3Bi with a purity of 98.9%2O3Na with a purity of 99.8%2CO3(ii) a Uniformly mixing all the weighed raw materials, putting the mixture into a nylon tank, fully mixing and ball-milling the mixture for 18 to 24 hours by taking zirconium balls as grinding balls and absolute ethyl alcohol as a ball-milling medium, separating the zirconium balls, drying the mixture of the raw materials for 24 to 36 hours at a temperature of between 80 and 100 ℃, grinding the mixture by using a mortar, and sieving the mixture by using a sieve of between 80 and 100 meshes;
(2) pre-firing
Placing the raw material mixture obtained in the step (1) in a quartz crucible, compacting by using a grinding rod, covering, pre-sintering for 3-4 hours at 850-900 ℃, naturally cooling to room temperature, and grinding by using a mortar to obtain pre-sintered powder;
(3) secondary ball milling
Putting the pre-sintering powder into a nylon tank, taking zirconium balls as grinding balls and absolute ethyl alcohol as a ball milling medium, fully mixing and ball milling for 18-24 hours, separating the zirconium balls, drying the pre-sintering powder for 24-36 hours at 80-100 ℃, grinding by using a mortar, and sieving by using a sieve of 180-200 meshes;
(4) tabletting
Pressing the pre-sintering powder sieved by a 180-200-mesh sieve into a cylindrical blank by using a powder tablet press, and then carrying out cold isostatic pressing for 15-20 minutes under the pressure of 200-300 MPa;
(5) pressureless closed sintering
And (3) placing the cylindrical blank on a zirconium oxide flat plate, placing the zirconium oxide flat plate in an alumina closed sagger, heating to 1160-1190 ℃ at the speed of 2-5 ℃/min, sintering for 1.5-3 hours, and naturally cooling to room temperature along with a furnace to prepare the sodium bismuth titanate-based ceramic material.
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